Method of producing lubricating oils



Mar. 13, 1923. I .l,448,084

' 11 F.(DTT

METHOD 0F PRODUCINQ .T'JUBRICATING OILS Filed May 1, 1920 Patented Mar.13, 1923.

UNITED STATES PATENT OFFICE.

THOMAS F. GT1, BERKELEY, CALIFORNIA.\

METHOD or PRODUCING LuBRIcA'rmGoILs.

the lubricating distillates or oils in sucha manner as to produce in asingle-cycle of operation the light'colored oils required or demanded bythe public, and which it is the desire of the manufacturer to supply,

1 but which heretofore has not been accomplished successfully except ata materialincrease in cost. The essential objectsjof the presentinvention are to produce light colored oils at a materially lessexpensethan under the former methods employed; to expedite themanufacture of such colored oils;

to successfully produce the desired light colored oils in a single cycleof operation and by so doing materially increasingthe daily output of aplant of given capacity, and todispense with the filtration of the oilthrough a. filtering medium of fullers earth, and which filtering stepis essen-' tial in such previous methods employed and generallyfollowedin all manufacturing plants for the production of light coloredoil-s.

ess of treating lubricating distillates or' oils for the production oflight color oils, embodied essentially the following steps. Firstagitating the distillate or oil with sulphuric acid, settling out andwithdrawing the sludge produced by the acid re-action; second, asubsequent agitation or spraying with a suitable neutralizing agent, forinstance,

sodium hydroxide, a settling out and withdrawal of the waste alkali andpossible followed in the order given constitutea single cycle operation,but the lubricating oil so produced was generally of a red colorv Priorto the present invention the. recognized and accepted standard methodor'procproducts of reaction; third, washing by agi- 1920. Serial No.378,094.

and in order to produce the pale or light colored oils in popular demandby the pub.-

lie for gasoline motors, it was required to,

carry the method a step farther, viz': filter the oil so producedthrough a decolorizing] agent,usually by passing the same through a tankor filter filled with fullers earth.

. Each manufacturer varied as desired the quantity of sulphuric acidused and neutralizi'ng agent employed and equally so the time periods oftreatment, but for a, full understanding of said standard method, the

following description is illustrative:

Approximately, seven hundred (700) barrels of lubricating distillatewereplaced in 4 an acid-agitator, a conical bottomed vessel having a holdingcapacity of about one thousandflOOO) barrels. The oil was then agitatedin the presence of about seventytwo :hundred (7200) pounds 'of 98%sulphurio acid added thereto, by means of com pressed air for a periodof approximately thirty (30) minutes. After agitation settlingwasallowed for approximately two hours and the sludge formed drawn. Theoil-was then subjected to a secondagitation with an additionalninety-seven hundred (9700) pounds of sulphuric acid for a period ofabout thirty minutes, settling allowed for sixteen hours and the sludgedrawn off as before. Agitation was again resorted to and an additionalthirty two hundred (320 pounds of acid was added and, at the expirationof thirty minutes 9 blowing with acid. water. was sprayed over thesurface of theoilv This, water is known as coking water and its additionduring agitation was tocollect and agglomerate the very fine particles'of sludge formed by the action of the acid on the oil, into particlesofsuch size as to settle out fairly easily. .No coking medium wasrequired during the two first agitations, due to the fact that the firsttwo increments of acid resulted in the formation of a sludge not sofinely divided and which consequently settled out with ease. Followingthe application of the coking medium, settling was allowed for one hour,the sludge drawn off and the oil transferred from the acid agitator intoan alkali agitator, similar in construction to the acid agitator. A hotsolutionof sodium hydroxide was sprayed onto the oil until about 160barrels had been added and settling was then allowed for two hours. Thewaste alkali and ossible reaction products were drawn and fresh alkaliadded until the oil was thoroughly neutralized. The alkali was settledout as well as possibleby standing about 16 hours and then drawn off.The oil was then washed by spraying on hot water to remove any traces ofalkali and the water settled out as perfectly as possible and drawn ofl'However, mere settlin not being sufficient' to. remove all traces omoisture, the

Oil a e h n transferred t a th s p lbwi-li'ctan'gulir. fin known as theblow w p'a oil was'heate'd 3 mean .of closed ste m coils and com;

pressedair pissed through it until the Oil was perfectly bright andfreefrom moisture. The resulting oil was generall of aired coleraiid'inorder to produce t e pale for ..light colored oils in popular demand forgasolineiniotors, it was necessary to filter this oil thrjough a tankfilled with fnllers earth, whi'ch isafdecoloriz'ing agent.

was e slow and expensive process and U at Various times t w s endeavoredto produce light colored .oils by increasing the amount of acid in thechemical treatment However, results were not encouragin and, in fact,the larger amounts or acif used seemed to result in an even darkerredoil in th l wrp i n en emp oy the larger vamounts of acid, additionswere always made in three increments, although the relative proportionsof th increments were varied, 'One coking water? waszilways used afterthe last increment of acid. ,Efl'orts were made to get a light coloredoil by'using. a larger amount of acid by taking the oil f om theblow-pan and putting it :back in the acid agitator and so subject it to,I a complete additional cycle of chemical treatmentnfl i i As the u al paf w ste give a treat of oil about 120,000 ounds of adder presticallyflthirtfy poun s of acidper barrel of oil thee i1. when putthrough two cycles not 1 'lfleivddm bl he amount 7 of acid, but also ofalkali and were, In the second cycle'tlie sludge formed by the action ofthe l acidwas less in amount than during the first the ,oil beingtreated with'each alkali wash,

added to the ,cost of thealkali and operating costs, make a two cycletreatment uncommercial, but'I am enabled by my invention to produce adecolorized. .oil economically and in a shorter period of time.

In order to produce the pale or light,

colored oil by a single cycle treatment and at the same time dispensewith the use of fullers earth filtration or other de-coloring agentafter treatment of the oils in thealkali agitator, I discovered thefollowing method of treatment, which will be readily understood byreference to the accompanying sheet of drawings wherein is representeddiagrammatically the movement of the oil through a single cycletreatment.

Theusual' amount of oil, about seven hundred barrels, is placed withinthe agitator 1 and during agitation si' bjected tothe action of fortythousand pounds of sulphui'ic a'cid,t'he acid being addedin four or fiveincrements. After the first increment of say, eight thousand pounds, theoil is agitated for'fifteen minute's, andsettling allowed for two hours.The slud e is then drawn ofi through the controlled outlet 2 of't'heagitator 1, and a second increment of eight thousand pounds of acidadded to the oil and, the same agitated for fifteen minutes, and allowedto settle for approximately sixteen hours before drawing oflt' thesludge- The oil is then subjected to a third agitation with eightthousand pounds of acid for a period f fifteen minutes and durg i'agitation treated with about seven barre. 0f coking water foragglomerating and collecting the small farticj es of sludge con tainedthere in ands lowed to settle for six hours. The oil i'sthen subjectedto two additional agitations, with each there being addd ightfthOusaI-idpounds of acid, the agitation and settling being as before, coking wateror other coking agent being spra edjonto the oil during each period ofagitation after the adding of the acid. It willbe understood that aftereach settling period the sludge formed by the acid r act on i r v 0 t,although th s ling between increments of acid is a variable fac tor dependent on the character of oil to be "treated. After subjecting the oilto the of the series of applications of coking water and withdrawal ofthe sludge, the

011 then need Ortrwu g formed by reactions of the sulphuric acid istransferred 'to an alkali agitator 3, similar in all respects to'the'agitator 1 and, as common in the art oftrea ting the oil sprayed with ahot solution of sodium hydroxide until about one "hundred and sixtybarrels are itddfidflfld; the oil fthen allowed ,toscttIe for about twohours, The waste alkali is drawn oi and alkali added until the oil istheroughly neutralized. vFrom this point on and in faetfrom thetime' oitransference of the oil into the a'llkali agitator, the method is ,the'san ieas that heretofore followed, except'tha't after treatment in theacidagitator the oil is not passed through fullers earth or subjected inany manner to decolo-rizing agents, su'ch'being rendered unnecessary byreason of the factthajt subjecting the oil to with filtration by theremoval from within the oil of the sludge formed by the reactions of thesulphuric acid} The severalcoking treatments or multiple-coking employedor utilized in my process permits of an increased amount of sul'-,

' phuric acid being utilized in one cycle of operation. 'lVhile the'useof water asa coking medium is specifically mentioned in the treatment ofthe oils, it will be understood that water is notessential as the cokingmedium, inasmuch as a weak solution of sodium hydroxideancl a. Weak acidsolution have been utilized by me with success, pro- Vided that thesolution of sodium hydroxide is dilute enough to have no appreciableneutralizing effect upon the mixture of oil and acid, and, therefore, bythe expression coking medium or coking agents as hereinafter employed,is meant to be understood the utilization of Water or any otherpermissible solution as the coking medium, but preferably I use Waterinasmuch as the use of weak sodium hydroxide or weak acid addsmaterially to the cost of the process without producing other beneficialresult by their use in the place of Water.

The use of the multiple coking employed in the step for eliminating thereaction products of the sulphuric acid is the simplest, cheapest andeasiest way for most completely removing the sludge formed in the acidagitator after each increment of acid.

It is essential that multiple coking be utilized in order that thereaction products of the acid employed in connection with one treatmentbe removed as completely as possible before adding fresh acid, for,otherwise, the increased amount of sulphuric acid tends to oxidize orburn the oil.

While the maximum amount of acid used in the carrying out of my methodis generally double that used in the former methods employed for thetreatment of the oils, or roughly sixty pounds of acid per barrel of oiltreated, yet the amount of acid is adjusted according to the degree ofcolor desired in the finished product, and experience has demonstratedthat quite a few of the oils do not require double the amount of acid tobe utilized in my single cycle operation, over the quantity of acidemployed in the carrying out of the former methods.

While the number and size of the increments of acid employed is notfixed, practical experiments have demonstrated that preferably theseshould be five in number, and While the coking treatment may be avariable one, the same should never be less than two in number.

Contrary to popular conception, the use of the additional amount ofsulphuric acid required in the carrying out of my process doesn'ot'result inaj smaller yield of the finished'lubricating oil, for thepercentage losses in'this process are no higher than in the formermethods employed;

-The invention desired to be protected resides in subjecting thedistillates or oils for treatment to a plurality of agitating periods,

each period being followed by a period of settlement and each period ofagitation being in the presence of a fixed quantity of sulphuric acidadded to the oil and subjecting the oil during certain successiveagitating treatment to the application of a coking medium, 'the' cokingmedium being applied to the oil during thesuccessive agitating periodsthereof, and in number the coking treatments of the oil being never lessthan two, whereby the oil is freed of the sludge formed by the acidreactions, so that when delivered from within the alkali agitator thesame is of the light color desired.

It will be understood that the foregoing description does notnecessarily represent, and is not intended to represent,- the exacttreatment for all oils under the present method invention, inasmuch asthe quantity of acid coking material, and the quantity and number ofacid increments should be varied in accordance with thecharacter of theoil to be treated or to be obtained.

Having thus described my invent-ion, what I claim as new and desire toprotect by Letters Patent is i 1. The method of treating oils for theproduction of light colored lubricating oils without subjecting the sameto the action of a decolorizing agent after the acid treatment thereof,the same consisting in subjecting the oil to successive periods ofagitation and settlement, adding a given quantity of sulphuric acid tothe oil during each period of agitation, and during a plurality of saidsuccessive agitations subjecting the-oil to the action of water for thecollecting and separation of the sludge formed by the acid reactions,thence subjecting the oil freed of the sludge to a treatment with analkali solution.

2. The process of decolorizing oils which consists in mixing acid withan oil by a number of increments, adding water to each oil and acidmixture after more than one of the acid increments, removing acid sludgeafter each acid increment, then washing with an alkali after removal ofthe acid sludge resulting from the final acid increment.

3. The process of decolorizing oils which consists in mixing acid withan oil by a number of increments, adding Water to each oil and acidmixture after the first two increments, removing acid sludge after eachacid increment, then Washing with an alkali after removal of the acidsludge resulting from the final acid increment.

t. The process of decolorizing oils which consists in mix-iug acid withan oil k five eman d n gw ea h? 1 1:;- -ure af ore t an Qne of th Mi d lrp ments, removing spud sludge after each gcyd increment, then washingwith an alkali aftpr ber of increments, adding Water to @3011 oil andacid mixture @fber more'than one oi e i iremen s; zem vingu id slndggafter each ac ncmm nmh n wasbi w th an alkali after removal of the acid11 e msulting from the final aci d treapment; {be number of acidincrementsbeing ppt lg hgm in and. 3m. umb r of WW a d finn f consistsin agiigting a lubricaiil, 011 With sulphuric acid, which aqid 3d 9d 1n.6 cesgive incremgnts, mixing main with the Oil d a d mixtur during thethir an sunwi a i wm ms mo i cupid sludge after eagh ipc rgment,131.1611 Washm with a alkal aftqr' m va o the 11? lllfl e esulting f mhe final id inc meat md d awing alka i w ste ,liquglrs- In m timhywhmfioi I have igned my name to thi spmifimtmn- THOMAS F. .OTT.

